EP0799809A2 - Composites à matrice céramique, leur procédé de préparation par infiltration en phase liquide de précurseurs céramiques polymériques et utilisation de poudres nanométriques - Google Patents

Composites à matrice céramique, leur procédé de préparation par infiltration en phase liquide de précurseurs céramiques polymériques et utilisation de poudres nanométriques Download PDF

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Publication number
EP0799809A2
EP0799809A2 EP97830161A EP97830161A EP0799809A2 EP 0799809 A2 EP0799809 A2 EP 0799809A2 EP 97830161 A EP97830161 A EP 97830161A EP 97830161 A EP97830161 A EP 97830161A EP 0799809 A2 EP0799809 A2 EP 0799809A2
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EP
European Patent Office
Prior art keywords
sic
nanometric
powders
ceramic
cloths
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EP97830161A
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German (de)
English (en)
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EP0799809B1 (fr
EP0799809A3 (fr
Inventor
Aldo Donato
Alberto Ortona
Carlo Alberto Nannetti
Elisabetta Borsella
Sabina Botti
Gianni D'alessandro
Sergio Casadio
Antonio Alessandro Licciulli
Stefano Martelli
Amedeo Masci
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Agenzia Nazionale per le Nuove Tecnologie lEnergia e lo Sviluppo Economico Sostenibile ENEA
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Agenzia Nazionale per le Nuove Tecnologie lEnergia e lo Sviluppo Economico Sostenibile ENEA
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Publication of EP0799809A3 publication Critical patent/EP0799809A3/fr
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
    • C04B35/571—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide obtained from Si-containing polymer precursors or organosilicon monomers
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/71—Ceramic products containing macroscopic reinforcing agents
    • C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
    • C04B35/80—Fibres, filaments, whiskers, platelets, or the like
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S977/00—Nanotechnology
    • Y10S977/70—Nanostructure
    • Y10S977/778—Nanostructure within specified host or matrix material, e.g. nanocomposite films
    • Y10S977/779—Possessing nanosized particles, powders, flakes, or clusters other than simple atomic impurity doping
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S977/00—Nanotechnology
    • Y10S977/84—Manufacture, treatment, or detection of nanostructure
    • Y10S977/842—Manufacture, treatment, or detection of nanostructure for carbon nanotubes or fullerenes
    • Y10S977/847—Surface modifications, e.g. functionalization, coating
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S977/00—Nanotechnology
    • Y10S977/84—Manufacture, treatment, or detection of nanostructure
    • Y10S977/89—Deposition of materials, e.g. coating, cvd, or ald
    • Y10S977/891—Vapor phase deposition
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S977/00—Nanotechnology
    • Y10S977/84—Manufacture, treatment, or detection of nanostructure
    • Y10S977/89—Deposition of materials, e.g. coating, cvd, or ald
    • Y10S977/892—Liquid phase deposition
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S977/00—Nanotechnology
    • Y10S977/84—Manufacture, treatment, or detection of nanostructure
    • Y10S977/895—Manufacture, treatment, or detection of nanostructure having step or means utilizing chemical property
    • Y10S977/896—Chemical synthesis, e.g. chemical bonding or breaking
    • Y10S977/897—Polymerization
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S977/00—Nanotechnology
    • Y10S977/84—Manufacture, treatment, or detection of nanostructure
    • Y10S977/90—Manufacture, treatment, or detection of nanostructure having step or means utilizing mechanical or thermal property, e.g. pressure, heat
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S977/00—Nanotechnology
    • Y10S977/902—Specified use of nanostructure
    • Y10S977/961—Specified use of nanostructure for textile or fabric treatment

Definitions

  • the present invention relates to the production of a ceramic matrix composite (CMC) reinforced by fibres of the ceramic type.
  • CMC ceramic matrix composite
  • CMCs are a class of technologically advanced materials which have been increasingly developed in recent years for industrial applications in leading sectors such as aerospace, energy, and automobile industry due to their very high mechanical strength, chemical inertness and heat resistance along with their further feature of lightness.
  • studies for the application of such materials in the construction of the future controlled thermonuclear fusion reactors are being conducted in USA, Japan and Europe.
  • the basic mechanical characteristic of CMCs is the capability of breaking under loaded conditions in a not catastrophic manner unlike the monolithic ceramic materials of fragile nature for which the design of structural components is very difficult.
  • the reason of such an advantageous mechanical behaviour of CMCs is the deflection of the cracks caused in the ceramic matrix by a thermal or mechanical stress to the direction of the fibre-matrix interphase.
  • CMC Ceramic Vapor Infiltration
  • the gases decompose in the furnace forming in the ceramic fibre materials the ceramic matrix which is formed of silicon carbide (SiC) in case of SiC/SiC fibre CMC.
  • the decomposition of the gases should be carried out slowly according to a determined kinetics allowing a complete infiltration, preferably from the inside of the material, which then requires a very long time in the order of several months for the construction of 5-6 mm thick pieces.
  • Products having mechanical characteristics fully satisfying the specification required for their use are provided by such a process.
  • the process suffers from not negligible troubles, particularly as far as the production cost is concerned which is very high above all because of the very long production time.
  • the precursor changes into the ceramic matrix by a thermal pyrolysis treatment, bounding the fibres and having an amorphous or nanocrystalline structure according to the pyrolysis temperature by a thermal pyrolysis treatment.
  • a considerable loss of weight of the precursor 25-40%) takes place because of evaporation of oligomers and structural rearranging with evolution of gases such as methane, other hydrocarbons and hydrogen.
  • Such powders are resorted to because they allow the voids in the fibre materials and among the material layers to be better filled so as to reduce the total number of the necessary infiltration and pyrolysis cycles in the whole process.
  • the currently used inert fillers are commercially available SiC powders of micrometric granulometry.
  • Such powders suffer, however, from further problems among which the not homogeneous distribution of the same as the powder particles hardly enter the fibre bundles (typically formed of 500-1000 fibres of 5-15 ⁇ m diameter), the gaps among the fibres being by two orders of magnitude narrower than the size of the fibres.
  • the amorphous or nanocrystalline nature of the matrix produced by the pyrolysis of preceramic polymers can be affected by the presence of crystalline particles having much larger size, thus impairing the mechanical characteristics.
  • a CMC having improved mechanical characteristics, particularly as far as density and homogeneity of the matrix is concerned is still expected. It is also important for the industry that such a material can be produced with industrially interesting time and cost as well as with large enough thickness so as to be used, for instance, as structural component in large plants.
  • One object of the present invention is to overcome the problems of the known CMCs and processes for the production thereof.
  • Such object is achieved according to the invention by manufacturing CMCs of high density, preferably of the SiC/SiC type, by a production process based on the infiltration into ceramic fibre materials of a polymeric precursor solution containing, as filler, inert powders of much lower size than the mean distance among the ceramic fibres used as basic materials for the manufacturing of CMCs and typically having a nanometric granulometry.
  • Such infiltration step is followed by the steps of material hardening and polymer pyrolysis, and by repeated thickening steps until the desired density is reached.
  • Polycarbosilane is a general term indicating a class of organic silicon polymers which produce a ceramic SiC residue as a result of a pyrolysis treatment at a temperature T > 800°C under controlled atmosphere.
  • SiC fibres are of the type commercially known as Nicalon (Nippon Carbide, Japan) which are carbon coated, i.e. have a surface deposit of pyrolytic carbon of a typical thickness of 0,1-1 ⁇ m and a diameter approximately of 15 ⁇ m.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Ceramic Products (AREA)
EP97830161A 1996-04-05 1997-04-04 Composites à matrice céramique Expired - Lifetime EP0799809B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
IT96RM000220A IT1284620B1 (it) 1996-04-05 1996-04-05 Compositi a matrice ceramica, e processo di produzione degli stessi mediante infiltrazione liquida con precursori ceramici polimerici e
ITRM960220 1996-04-05

Publications (3)

Publication Number Publication Date
EP0799809A2 true EP0799809A2 (fr) 1997-10-08
EP0799809A3 EP0799809A3 (fr) 1998-01-14
EP0799809B1 EP0799809B1 (fr) 2001-07-25

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ID=11404079

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Application Number Title Priority Date Filing Date
EP97830161A Expired - Lifetime EP0799809B1 (fr) 1996-04-05 1997-04-04 Composites à matrice céramique

Country Status (4)

Country Link
US (1) US5853653A (fr)
EP (1) EP0799809B1 (fr)
DE (1) DE69705761D1 (fr)
IT (1) IT1284620B1 (fr)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0941926A3 (fr) * 1998-03-09 2000-03-01 MAN Technologie AG Composants constructifs mobiles pour un dispositif sous charge thermo-mécanique et méthode pour leur production
EP1024121A3 (fr) * 1999-01-28 2001-01-10 Ishikawajima-Harima Heavy Industries Co., Ltd. Elément composite à base de céramique et sa méthode de fabrication
EP1081115A1 (fr) * 1999-09-06 2001-03-07 Ishikawajima-Harima Heavy Industries Co., Ltd. Procédé et appareil pour la fabrication d'un corps composite à base de ceramique
EP1591429A1 (fr) * 2004-04-19 2005-11-02 Erbicol SA Mousse céramique à cellules ouvertes avec des cavitées rondes et procédé de fabrication

Families Citing this family (22)

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US6735842B1 (en) * 1999-03-08 2004-05-18 Man Technologie Ag Movable structural component for a thermomechanically stressed assembly as well as a process for producing the structural component
US6441341B1 (en) 2000-06-16 2002-08-27 General Electric Company Method of forming cooling holes in a ceramic matrix composite turbine components
US6630029B2 (en) * 2000-12-04 2003-10-07 General Electric Company Fiber coating method and reactor
DE10204860A1 (de) * 2002-02-06 2003-08-14 Man Technologie Gmbh Faserverbundkeramik mit hoher Wärmeleitfähigkeit
US7628942B1 (en) 2006-04-25 2009-12-08 The United States Of America As Represented By The United States Department Of Energy Resin infiltration transfer technique
US8101272B1 (en) * 2006-06-16 2012-01-24 United Technologies Corporation Armor shell and fabrication methods
PT2522299T (pt) * 2011-05-10 2020-10-20 Harald E Nordin Implante dentário
PL2522300T3 (pl) 2011-05-10 2021-06-28 Peter Nordin Wspornik do implantu dentystycznego
US9764987B2 (en) 2012-03-02 2017-09-19 Dynamic Material Systems, LLC Composite ceramics and ceramic particles and method for producing ceramic particles and bulk ceramic particles
US10399907B2 (en) * 2012-03-02 2019-09-03 Dynamic Material Systems, LLC Ceramic composite structures and processing technologies
KR101540306B1 (ko) * 2013-10-21 2015-07-30 경희대학교 산학협력단 탄화규소 복합체(SiCf/SiC)의 제조방법
EP3063104A4 (fr) * 2013-10-30 2017-07-19 United Technologies Corporation Article en céramique et procédé associé faisant appel à l'infiltration de particules et à l'infiltration d'un polymère pré-céramique
US9624138B2 (en) 2014-04-08 2017-04-18 United Technologies Corporation Formation of voids within components formed from porous substrates
AU2015322020B2 (en) * 2014-09-22 2020-10-15 Georgia Tech Research Corporation Composite nanoparticle stabilized core carbon molecular sieve hollow fiber membranes having improved permeance
US10086544B2 (en) 2015-10-09 2018-10-02 United Technologies Corporation Laminate resin transfer molding of fibrous preforms using particle filled resin systems
US10472713B2 (en) 2016-05-31 2019-11-12 United Technologies Corporation Method for ceramic matrix composite with carbon coating for wetting
WO2018102352A1 (fr) * 2016-11-29 2018-06-07 Free Form Fibers, Llc Fibre ayant un ou plusieurs additifs élémentaires et procédé de fabrication
US11780780B2 (en) * 2017-03-20 2023-10-10 United States Of America As Represented By The Secretary Of The Air Force Oxidation-resistant fiber coatings and related methods
US10730203B2 (en) 2017-09-22 2020-08-04 Goodman Technologies LLC 3D printing of silicon carbide structures
US11274066B1 (en) 2017-11-30 2022-03-15 Goodman Technologies LLC Ceramic armor and other structures manufactured using ceramic nano-pastes
BR112020014259A2 (pt) * 2018-01-19 2020-12-01 Albany Engineered Composites, Inc. método de fabricação de um compósito de matriz cerâmica
CN114907127B (zh) * 2022-05-09 2023-04-28 厦门大学 一种基体改性的SiC/SiC复合材料及其制备方法

Citations (3)

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Publication number Priority date Publication date Assignee Title
EP0536866A1 (fr) * 1991-10-11 1993-04-14 Noritake Co., Limited Matériau nanocomposite renforcé par fibre de carbone à base de nitrure de silicium et procédé de sa production
EP0626360A1 (fr) * 1993-05-24 1994-11-30 Societe Europeenne De Propulsion Procédé de fabrication d'un matériau composite à interphase en carbone pyrolytique de microtexture lamellaire entre fibres de renfort et matrice, et matériau tel qu'obtenu par le procédé
WO1995035268A1 (fr) * 1994-06-17 1995-12-28 United Technologies Corporation Materiau composite resistant a des temperatures elevees et obtenu a partir de poudres a nanostructures

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US4837230A (en) * 1987-05-07 1989-06-06 Kaiser Aerotech Structural ceramic materials having refractory interface layers
JP2735151B2 (ja) * 1994-11-15 1998-04-02 工業技術院長 繊維強化炭化ケイ素複合セラミックス成形体の製造方法

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0536866A1 (fr) * 1991-10-11 1993-04-14 Noritake Co., Limited Matériau nanocomposite renforcé par fibre de carbone à base de nitrure de silicium et procédé de sa production
EP0626360A1 (fr) * 1993-05-24 1994-11-30 Societe Europeenne De Propulsion Procédé de fabrication d'un matériau composite à interphase en carbone pyrolytique de microtexture lamellaire entre fibres de renfort et matrice, et matériau tel qu'obtenu par le procédé
WO1995035268A1 (fr) * 1994-06-17 1995-12-28 United Technologies Corporation Materiau composite resistant a des temperatures elevees et obtenu a partir de poudres a nanostructures

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0941926A3 (fr) * 1998-03-09 2000-03-01 MAN Technologie AG Composants constructifs mobiles pour un dispositif sous charge thermo-mécanique et méthode pour leur production
US6673402B2 (en) 1998-03-09 2004-01-06 Man Technologies Ag Fiber-reinforced ceramics in spacecrafts and aerodynes
EP1024121A3 (fr) * 1999-01-28 2001-01-10 Ishikawajima-Harima Heavy Industries Co., Ltd. Elément composite à base de céramique et sa méthode de fabrication
US6368663B1 (en) 1999-01-28 2002-04-09 Ishikawajima-Harima Heavy Industries Co., Ltd Ceramic-based composite member and its manufacturing method
EP1081115A1 (fr) * 1999-09-06 2001-03-07 Ishikawajima-Harima Heavy Industries Co., Ltd. Procédé et appareil pour la fabrication d'un corps composite à base de ceramique
US6723381B1 (en) 1999-09-06 2004-04-20 Ishikawajima-Harima Heavy Industries Co., Ltd. Method and apparatus for manufacturing ceramic-based composite member
EP1591429A1 (fr) * 2004-04-19 2005-11-02 Erbicol SA Mousse céramique à cellules ouvertes avec des cavitées rondes et procédé de fabrication

Also Published As

Publication number Publication date
ITRM960220A1 (it) 1997-10-05
ITRM960220A0 (fr) 1996-04-05
EP0799809B1 (fr) 2001-07-25
US5853653A (en) 1998-12-29
DE69705761D1 (de) 2001-08-30
EP0799809A3 (fr) 1998-01-14
IT1284620B1 (it) 1998-05-21

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